CN106706804B - Method that is a kind of while measuring six kinds of component contents in black canarytree leaf - Google Patents
Method that is a kind of while measuring six kinds of component contents in black canarytree leaf Download PDFInfo
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- CN106706804B CN106706804B CN201710131129.XA CN201710131129A CN106706804B CN 106706804 B CN106706804 B CN 106706804B CN 201710131129 A CN201710131129 A CN 201710131129A CN 106706804 B CN106706804 B CN 106706804B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The invention discloses a kind of methods for measuring six kinds of component contents in black canarytree leaf simultaneously, comprising the following steps: step 1: sample solution preparation: after black canarytree leaf drying and crushing, sample solution is obtained by filtration in constant volume after carrying out ultrasonic extraction to the black canarytree leaf after smashing；Step 2: preparation reference substance solution；Chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin in the reference substance solution containing known quantity；Step 3: sample solution, reference substance solution chromatography: can be calculated to the content of chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin in black canarytree leaf after high-efficient liquid phase chromatogram technique analysis.The purpose of the present invention is to provide a kind of methods for measuring six kinds of component contents in black canarytree leaf simultaneously, can more it is intuitive fast and effeciently measure black canarytree leaf main active, detection accuracy and accuracy are high, reproducible, provide strong scientific basis for the further exploitation of black canarytree leaf.
Description
Technical field
The present invention relates to the measurement fields of black canarytree leaf, and in particular to a kind of to measure in black canarytree leaf six kinds of component contents simultaneously
Method.
Background technique
Canarium pimela (Canarium pimela Leenh.) also known as black olive, Canarium primela are woody oleiferous plants and fruit with evergreen Qiao
Wood species belong to Burseraceae Canarium on plant classification, originate in South China of China, are distributed widely in the Southeast Asia such as Vietnam
Country, root, leaf, kernel can be used as medicine, civil to be often used for treatment lumbago, skelalgia of rheumatism, numb in every limb, stomachache, burn.
Black canarytree leaf is simple and easy to get, high financial profit.In this seminar early-stage study, by isolated rat vascular circle perfusion,
The methods of arteria carotis intubation and Perfused isolated heart, discovery canarium pimela leaf extract has quickly short-acting antihypertensive effect, and it is dropped
Pressure effect and duration improve and extend with the increase of drug dose；It also has apparent reducing heart rate, steady simultaneously
The effect of the cardiovascular aspects such as fixed and increase coronary flow.
Exist to have in result of study prompt canarium pimela leaf extract and acts on cardiovascular active material, and in constituent analysis
Aspect, the existing research to black canarytree leaf is reported mainly on volatile oil, and other chemical constitution studies temporarily have no relevant report,
There is large stretch of blank in material base.
In addition, a large amount of research shows that chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin both at home and abroad
The bioactivity such as anti-oxidant, anticancer, protection cardiovascular system are all had, there is potential applications well prospect.In assay
Aspect, not yet disclose at present record and meanwhile measure chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin this six
The high performance liquid chromatography of kind component content.
Summary of the invention
The invention discloses a kind of methods for measuring six kinds of component contents in black canarytree leaf simultaneously, specifically, this six kinds at
It is divided into chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin, method of the invention more intuitive can quickly have
The main active of effect ground measurement black canarytree leaf, detection accuracy and accuracy are high, reproducible, are the further exploitation of black canarytree leaf
Strong scientific basis is provided.
A kind of method measuring six kinds of component contents in black canarytree leaf simultaneously provided by the invention, comprising the following steps:
Step 1: sample solution preparation: after black canarytree leaf drying and crushing, after carrying out ultrasonic extraction to the black canarytree leaf after smashing
Sample solution is obtained by filtration in constant volume；
Step 2: preparation reference substance solution；It is chlorogenic acid, Vitexin in the reference substance solution containing known quantity, different male
Jing Su, Hyperoside, rutin and Quercetin；
Step 3: chromatography: sample solution, reference substance solution can be calculated after high-efficient liquid phase chromatogram technique analysis
Obtain the content of chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin in black canarytree leaf；
Wherein, the chromatographic condition of high performance liquid chromatography are as follows: chromatographic column be C-18 chromatographic column, 250*4.6mm, 5 μm；Flow velocity
For 1mL/min；
Detection wavelength is 360nm；Column temperature is 30 DEG C；Sampling volume is 20 μ L；Mobile phase is -0.4% phosphoric acid of methanol, gradient
Elution；Using quantified by external standard method, chromatogram record is completed with processing by work station, and theoretical cam curve is calculated by chlorogenic acid peak, no
Lower than 8000.
It should be noted that above-mentioned step 1 specifically:
By black canarytree leaf drying and crushing, No. two sieves are crossed；
For accurately weighed black canarytree leaf powder 0.5g in stuffed conical flask, the methanol-water that percentage by volume is 50% is added in precision
Solution 50mL, close plug impregnate ultrasound 30min after 30min, stand cooling；
The methanol aqueous solution that percentage by volume is 50% is added and supplies weightlessness, shakes up, filters；Take subsequent filtrate cross 0.22 μm it is micro-
Hole filter membrane is to get sample solution.
It should be noted that above-mentioned step 2 specifically: accurately weighed chlorogenic acid, Vitexin, isovitexin, Hypericum Chinense
Glycosides, rutin and Quercetin reference substance are appropriate, and the methanol aqueous solution ultrasonic dissolution that percentage by volume is 50% is added, and constant volume shakes up,
Up to mixed reference substance solution.
It should be noted that above-mentioned gradient elution method particularly includes: the percentage by volume of 0~8min, methanol is
23%~32% -0.4% phosphoric acid solution of methanol；8~30min, the methanol-that the percentage by volume of methanol is 32%~35%
0.4% phosphoric acid solution；30~50min, -0.4% phosphoric acid solution of methanol that the percentage by volume of methanol is 35%~70%；50~
55min, -0.4% phosphoric acid solution of methanol that the percentage by volume of methanol is 70%~23%；55~60min, the volume hundred of methanol
- 0.4% phosphoric acid solution of methanol that score is 23%~23%.
It should be noted that above-mentioned C-18 chromatographic column is ZorbaxSB-C18Chromatographic column.
It should be noted that the model DionexUltiMate3000 high-efficient liquid phase color of above-mentioned high performance liquid chromatograph
Spectrometer and Agilent1260 high performance liquid chromatograph；The model BSA224S electronic balance of the electronic balance, purchased from match
More this scientific instrument (Beijing) Co., Ltd of benefit；The model KQ-300DA ultrasonic cleaner of ultrasonic cleaner is purchased from elder brother
Ultrasonic instrument Co., Ltd of mountain city.
It should be noted that (Rutin, lot number 100080-201409, purity 91.9% supply the reference substance rutin
HPLC measurement) and Quercetin (Quercetin, lot number 100081-201408, purity 99.1% for HPLC measure) purchased from China eat
Product drug assay research institute.
It should be noted that chlorogenic acid (Chlorogenicacid, lot number PCS0348-150511, the purity
99.37%), Vitexin (Vitexin, lot number PCS0646-151102, purity 98.84%), isovitexin (Isovitexin,
Lot number PCS0647-151204, purity 98.47%) and Hyperoside (Hyperin, lot number PCS0522-150615, purity
98.28%) it is purchased from Chengdu Zhi Biaohuachun Bioisystech Co., Ltd.
It should be noted that the black canarytree leaf medicinal material is picked from Zhongshan City, Guangdong Province, by Guangdong pharmaceutical university Chinese medicine mark
This shop professor Liu Jizhu is accredited as the dry leaves of Burseraceae Canarium canarium pimela.
It should be noted that the methanol, acetonitrile are chromatographically pure, it is purchased from U.S. LABSCIENCE company, water is ultrapure
Water is purchased from Watson company；Phosphoric acid is that analysis is pure, is purchased from Tianjin Zhi Yuan chemical reagent Co., Ltd；Other reagents are point
It analyses pure.
The present invention is compared with the traditional method, and is had the advantage that
1. the present invention is compared by ultra high efficiency liquid phase-mass spectrometric hyphenated technique (UPLC/MS) using reference substance,
The database retrievals such as Scifinder, chemspider and Massbank, from black canarytree leaf first identified gone out including chlorogenic acid,
The liposoluble ingredients such as Vitexin, isovitexin, Hyperoside, rutin and Quercetin.By polyamide rough segmentation, collection contains
Chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and quercetin component eluent and carry out in vitro zoopery, send out
Existing its has the function of diastole rat chest aorta smooth muscle.
2. six ingredient separative efficiencies are high, it can reach baseline separation；
3. in the linear range, the linear relationship of 6 ingredients is good, sample recovery rate and relative standard deviation meet
" Chinese Pharmacopoeia " relevant regulations show that this method has good reliability and accuracy.
4. the requirement that withinday precision, day to day precision, repeatability and Intermediate precision can reach pharmacopeia relevant regulations.
5. chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin are established for the first time while being measured to this method
The high performance liquid chromatography of six ingredients, and be used successfully to quickly detect its content in black canarytree leaf, it can be more intuitive quick
The quality of black canarytree leaf is evaluated, provides strong scientific basis for the further exploitation of black canarytree leaf.
Detailed description of the invention
Fig. 1 is chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and the Quercetin mixing of the embodiment of the present invention 1
The high-efficient liquid phase chromatogram of reference substance solution；
Fig. 2 is the high-efficient liquid phase chromatogram of the canarium pimela leaf extract of the embodiment of the present invention 1.
Specific embodiment
With reference to embodiment, claim of the invention is described in further detail, but do not constituted
Any limitation of the invention, the modification of anyone limited times made within the claims in the present invention protection scope, still exists
Within the claims in the present invention protection scope.
Embodiment 1
The preparation of 1 sample solution
By black canarytree leaf drying and crushing, No. two sieves are crossed.In stuffed conical flask, precision adds accurately weighed black canarytree leaf powder 0.5g
Enter 50% methanol aqueous solution (V/V) 50mL, close plug impregnates ultrasound 30min after 30min, stands cooling, weighing.50% methanol is added
Aqueous solution (V/V) supplies weightlessness, shakes up, filtering.Subsequent filtrate is taken to cross 0.22 μm of miillpore filter to get sample solution.
2. prepared by reference substance solution
Accurately weighed chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin reference substance are appropriate, are added
50% methanol aqueous solution (V/V) ultrasonic dissolution, constant volume shake up to get mixed reference substance solution.
3. chromatographic condition
Chromatographic column is AgilentZorbaxSB-C18(250*4.6mm, 5 μm)；Flow velocity is 1mL/min；
Detection wavelength is 360nm；Column temperature is 30 DEG C；Sampling volume is 20 μ L；
Mobile phase is made of 0.4% phosphate aqueous solution (A) and methanol (B), and elution process is as follows: 0~8min, 23%~
32%B；8~30min, 32%~35%B；30~50min, 35%~70%B；50~55min, 70%~23%B；55~
60min, 23%~23%B.
4. the foundation and verifying of six kinds of component content measuring methods in black canarytree leaf
(1) linear, range, quantitative limit and detection limit
Mixing reference substance stock solution is taken, a series of standard solution of concentration is diluted to, measures peak face by the above chromatographic condition
Product obtains the linear regression side of 6 ingredients of black canarytree leaf as shown in Figure 1, with concentration X (μ g/mL) to peak area Y progress linear regression
Journey.
Mixed reference substance solution is repeatedly diluted, is analyzed, the minimum detection limit (LOD) of each ingredient and minimum fixed is obtained
Amount limit (LQD).When minimum detection limit and minimum quantitative limit are defined as signal-to-noise ratio and are respectively equal to 3 (S/N=3) and 10 (S/N=10)
Corresponding sample introduction concentration.
Experimental result is as shown in table 1 and Fig. 2, and in the linear range, linear relationship is good for 6 kinds of ingredients.
1 range of linearity of table, detection limit and quantitative limit measurement result
(2) precision test
The investigation of precision be measure mixed reference substance solution in a few days, day to day precision.Withinday precision is same
To same reference substance solution METHOD FOR CONTINUOUS DETERMINATION 6 times in it, and day to day precision is to survey one every 12 hours to same reference substance solution
It is secondary, it is continuous to survey 3 days.Each component content in mixing reference substance is calculated, its precision is evaluated with relative standard deviation.
Experimental result is as shown in table 2,6 kinds of ingredients of the measuring method it is in a few days equal with the relative standard deviation of day to day precision
The relevant regulations for meeting pharmacopeia illustrate that instrument precision is good.
In table 2 days and day to day precision tests measurement result
(3) repetitive test
It takes with a collection of 6 parts of medicinal material of black canarytree leaf, is prepared by above-mentioned sample solution preparation method, by above-mentioned chromatographic condition
Each component content in medicinal material is measured, its repeatability is evaluated with relative standard deviation.
Experimental result is as shown in table 3, and the RSD of 6 kinds of ingredients of measuring method meets the relevant regulations of pharmacopeia, illustrates foundation
Method repeatability is good.
3 repetitive test measurement result of table
(4) Intermediate precision is tested
It takes with a collection of black canarytree leaf medicinal material, is prepared by above-mentioned sample solution preparation method by different operation personnel, and
Respectively in DionexUltiMate3000 and Agilent1260 liquid phase, contain by each ingredient in above-mentioned chromatographic condition measurement medicinal material
Amount, relative standard deviation evaluate in-between precision.
Experimental result is as shown in table 4, and the RSD of 6 kinds of ingredients of measuring method meets the relevant regulations of pharmacopeia, illustrates foundation
Method precision is good.
4 Intermediate precision of table tests measurement result
(5) stability test
Black canarytree leaf medicinal material is taken, is prepared by above-mentioned sample solution preparation method, respectively in 0h, 2h, 4h, 8h, 16h,
For 24 hours, 36h and 48h evaluates its stability by each component content in above-mentioned chromatographic condition measurement sample with relative standard deviation.
Experimental result is as shown in table 5, and the RSD of 6 kinds of ingredients of measuring method meets the relevant regulations of pharmacopeia, illustrates that sample exists
It is interior for 24 hours at room temperature to stablize.
5 stability test measurement result of table
(6) sample recovery rate is tested
Precision weighs 6 parts of black canarytree leaf medicinal material of known content, every part of about 0.25g.It is separately added into a certain amount of mixing control
Product solution, is prepared by sample solution preparation method, by each component content in above-mentioned chromatographic condition measurement sample, calculating side
The method rate of recovery.
Experimental result is as shown in table 6, and the sample recovery rate of this method meets the related rule of pharmacopeia within the scope of 94-103%
It is fixed, show that this method has good reliability and accuracy.
6 sample recovery rate of table tests measurement result
Embodiment 2
Using high performance liquid chromatography of the present invention, to the chlorogenic acid in 10 batches of black canarytree leafs, Vitexin, different Vitex negundo var cannabifolia
This six kinds of ingredients of element, Hyperoside, rutin and Quercetin are carried out while being measured.
Experimental result is as shown in table 7:
Test result shows black canarytree leaf Content of Chlorogenic Acid ingredient relative amount highest, the black canarytree leaf of different batches, chlorogenic acid,
This six kinds of component contents of Vitexin, isovitexin, Hyperoside, rutin and Quercetin are different.The present invention establishes simple and effective
Content assaying method is conducive to more preferably control canarium pimela leaf quality, and for it, further exploitation provides test basis.
Above-described is only presently preferred embodiments of the present invention, all made within the scope of the spirit and principles in the present invention
What modifications, equivalent substitutions and improvements etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of method for measuring six kinds of component contents in black canarytree leaf simultaneously, which comprises the following steps:
Step 1: sample solution preparation: after black canarytree leaf drying and crushing, to constant volume after the black canarytree leaf progress ultrasonic extraction after smashing
Sample solution is obtained by filtration；
Step 2: preparation reference substance solution；Chlorogenic acid, Vitexin, different Vitex negundo var cannabifolia in the reference substance solution containing known quantity
Element, Hyperoside, rutin and Quercetin；
Step 3: chromatography: sample solution, reference substance solution can be calculated after high-efficient liquid phase chromatogram technique analysis
The content of chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin in black canarytree leaf；
Wherein, the chromatographic condition of high performance liquid chromatography are as follows: chromatographic column is C-18 chromatographic column, specification 250*4.6mm, 5 μm；Stream
Speed is 1mL/min；
Detection wavelength is 360nm；Column temperature is 30 DEG C；Sampling volume is 20 μ L；Mobile phase is -0.4% phosphoric acid of methanol, and gradient is washed
It is de-: 0~8min, -0.4% phosphoric acid solution of methanol that the percentage by volume of methanol is 23%~32%；8~30min, the body of methanol
- 0.4% phosphoric acid solution of methanol that product percentage is 32%~35%；30min~50min, the percentage by volume of methanol are 35%
~70% -0.4% phosphoric acid solution of methanol；50~55min, the methanol -0.4% that the percentage by volume of methanol is 70%~23%
Phosphoric acid solution；55~60min, -0.4% phosphoric acid solution of methanol that the percentage by volume of methanol is 23%~23%；Using external standard
Standard measure, chromatogram record are completed with processing by work station, and theoretical cam curve is calculated by chlorogenic acid peak, is not less than 8000.
2. method that is according to claim 1 while measuring six kinds of component contents in black canarytree leaf, which is characterized in that described
Step 1 specifically:
By black canarytree leaf drying and crushing, No. two sieves are crossed；
For accurately weighed black canarytree leaf powder 0.5g in stuffed conical flask, the methanol aqueous solution that percentage by volume is 50% is added in precision
50mL, close plug impregnate ultrasound 30min after 30min, stand cooling；
The methanol aqueous solution that percentage by volume is 50% is added and supplies weightlessness, shakes up, filters；Subsequent filtrate is taken to cross 0.22 μm of micropore filter
Film is to get sample solution.
3. method that is according to claim 1 while measuring six kinds of component contents in black canarytree leaf, which is characterized in that described
Step 2 specifically: accurately weighed chlorogenic acid, Vitexin, isovitexin, Hyperoside, rutin and Quercetin reference substance are appropriate, add
Enter the methanol aqueous solution ultrasonic dissolution that percentage by volume is 50%, constant volume shakes up to get mixed reference substance solution.
4. method that is according to claim 1 while measuring six kinds of component contents in black canarytree leaf, which is characterized in that described
C-18 chromatographic column is ZorbaxSB-C18Chromatographic column.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104076099A (en) * | 2013-03-29 | 2014-10-01 | 成都康弘药业集团股份有限公司 | Method for detection and quality control of medicine composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104076099A (en) * | 2013-03-29 | 2014-10-01 | 成都康弘药业集团股份有限公司 | Method for detection and quality control of medicine composition |
Non-Patent Citations (2)
| Title |
|---|
| Simultaneous detection of flavonoids and phenolic acids in Herba Lysimachiae and Herba Desmodii Styracifolii using liquid chromatography tandem mass spectrometry;Dongxiao Sun 等;《Food Chemistry》;20121102;第138卷(第1期);第139-147页 * |
| 广金钱草总黄酮纯化工艺优化及总黄酮提取物的抗氧化活性、定性和定量研究;郭盼盼;《中国优秀硕士学位论文全文数据库 医药卫生科技辑》;20160315(第03期);第83-85页 * |
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